CN108355669B - 一种磁性纳米洋葱碳负载Bi2WO6的光催化剂及其制备方法和应用 - Google Patents
一种磁性纳米洋葱碳负载Bi2WO6的光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种磁性纳米洋葱碳负载Bi2WO6的光催化剂及其制备方法和应用。本发明以磁性纳米洋葱碳(MCNOs)为载体,采用水热方法,制备出磁性Bi2WO6/MCNOs复合光催化剂。本发明的原料价廉易得、制备工艺简单;制备的复合光催化剂担载均一、活性组分不易脱落、稳定性高、不会对环境造成二次污染;且所得复合光催化剂在可见光条件下对目标污染物能高效吸附、矿化;纳米洋葱碳在极大程度上抑制了Bi2WO6光催化剂光生电子~空穴的复合,从而提高了催化剂的光催化活性,有效解决了光催化技术在实际应用中量子产率低的困难;该催化剂的分离回收更加便捷、高效,有望解决光催化粉末在悬浮体系中难以回收的问题。
Description
技术领域
本发明涉及一种磁性纳米洋葱碳负载Bi2WO6的光催化剂及其制备方法和应用,属于光催化剂及其制备技术领域。
背景技术
近年来,由于环境问题日益严重,能源日益紧缺,开发清洁能源对环境污染进行治理迫在眉睫,光催化技术因其在解决能源短缺和环境污染问题方面的潜在应用而受到国内外广泛关注。传统的光催化材料一般采用较大带隙的金属氧化物或硫化物,在实际应用中有以下不足之处:(1)光响应范围窄;作为传统半导体光催化剂的TiO2的禁带宽度为3.2eV,只能在紫外光区(只占太阳光能力的4%)有光催化活性;(2)量子产率低;由于材料本身的限制,光生电子~空穴数量较少或者易于复合;(3)催化剂分离回收性能差;传统光催化颗粒在液相中难以回收,使其应用受到极大限制。因此,如何研制高活性、宽谱响应且易于固液分离的光催化材料,是推进光催化技术在污染控制领域中广泛应用的前提和关键。
钨酸铋(Bi2WO6)是具有钙钛矿板的层状结构,价带是由Bi6s和O2p轨道杂化而成,轨道间的强相互作用降低了对称性产生相关的偶极子,使其具有更广的可见光波长响应、较高的氧化活性和电荷流动性。然而,现有的Bi2WO6材料在环境应用中还存在两大难题,一是催化剂分离回收较为困难;二是光生量子产率低,光生电子-空穴易复合导致降解效率低,因而需要对现有Bi2WO6进一步研究改进,以获得易回收且效率高的光催化材料。
发明内容
本发明旨在提供一种磁性纳米洋葱碳负载Bi2WO6的光催化剂及其制备方法和应用,通过将窄带隙的Bi2WO6活性组分负载在磁性纳米洋葱碳载体上,提高可见光吸收性能和固液分离回收性能。
本发明采用磁性纳米洋葱碳(Magnetic Carbon Nano Onions, MCNOs),这是一种新型的纳米材料,其独特的中空结构为电子的传输提供了通道;较大的比表面积也可加强染料的吸附和离子交换性能,加速有机染料的降解;此外,带有Fe-Ni核的CNOs的饱和磁化强度良好,能够实现催化剂与染料的磁性分离。因而,MCNOs是极好的催化剂载体,可提高光催化剂的降解效率并实现对光催化剂的磁性回收。
本发明提供了一种磁性纳米洋葱碳负载Bi2WO6的光催化剂,以Bi2WO6为活性组分,以磁性纳米洋葱碳为载体,将Bi2WO6活性组分负载在磁性纳米洋葱碳载体上形成;该催化剂包括以下重量份数的组分:
磁性纳米洋葱碳MCNOs:10~20wt%,
Bi2WO6:80~90wt%。
本发明提供了上述磁性纳米洋葱碳负载Bi2WO6的光催化剂的制备方法,包括以下步骤:
(1)将Bi(NO3)3·5H2O溶于硝酸中形成透明溶液A(2.5~3.5mmol/L),再将Na2WO4·2H2O溶于去离子水中形成透明溶液B(1.25~1.75mmol/L),其中,将Bi(NO3)3·5H2O与Na2WO4·2H2O的摩尔比为1.5:1~2:1;
(2)将溶液B以1~2mL/min的速度逐滴加入到溶液A中,形成白色悬浊液,用NaOH调节pH,磁性搅拌25~35min;
(3)取0.11~0.21g MCNOs加入到30-50mL表面活性剂中,超声分散25~35min,形成MCNOs分散液;
(4)将分散好的MCNOs分散液加入步骤(2)所得的悬浊液中,磁性搅拌25~35min;
(5)将上述溶液转入有聚四氟乙烯内衬的高温高压反应釜中,在烘箱中进行水热反应;
(6)待反应釜冷却到室温后,取反应釜中的产物,用水和无水乙醇交替清洗、离心、干燥后即可得到磁性Bi2WO6/MCNOs催化剂。
作为优选的制备方案,步骤(2)中的pH应调节至1~3。
步骤(3)中所述MCNOs的量应为理论Bi2WO6质量的10%~20%。
步骤(3)中所述表面活性剂为乙二醇。
步骤(5)中所述的水热反应温度即烘箱温度设置为140~180°C,反应时间为1~6h。
步骤(6)中所述的清洗即为用去离子水和无水乙醇交替清洗3~5次;离心转速为6000~8000r/min,离心时间为8~10min;干燥方式为烘箱干燥,温度设置在60~80°C,干燥时间为6~8h。
本发明提供了上述磁性纳米洋葱碳负载Bi2WO6的光催化剂在可见光条件下催化降解有机染料中的应用。
所述有机染料为罗丹明B(RhB)。降解过程中,RhB的浓度为10mg/L,Bi2WO6/MCNOs复合催化剂的投加量为1.0~1.5g/L。
本发明所述的Bi2WO6/MCNOs复合催化剂对有机染料的去除率在2h内的去除率可达80%以上。
本发明所制备的复合材料具有超顺磁性,即可通过外加磁铁完成对催化剂的磁性回收。催化剂回收方便,有利于重复使用。
本发明的有益效果:
(1)本申请将光催化活性组分Bi2WO6负载到MCNOS表面上,一方面有效解决光催化过程中催化剂的流失问题,提高光催化剂的稳定性;另一方面利用载体的大比表面积提供较多的活性位点,为光催化体系提供更多的微化学反应场所,进而协同提高光催化活性。
(2)通过本发明制备的催化剂是一种易于磁性回收的高效光催化剂,与纯Bi2WO6相比,无论是吸附性能还是催化降解性能,该催化剂都有很大的提升。
(3)使用该光催化剂处理RhB,光反应2h即可完全降解水中的污染物,反应完成后,用磁铁即可完成催化剂的分离。
(4)通过该方法制备光催化剂,操作简单、易于实施,可在水污染治理中推广使用。
附图说明
图1为实施例1中Bi2WO6/MCNOs、MCNOs和Bi2WO6的XRD图谱;
图2为实施例1中Bi2WO6/MCNOs的SEM图和EDS图;
图3为实施例1中Bi2WO6/MCNOs和MCNOs的磁滞回线图;
图4为实施例1中Bi2WO6/MCNOs、MCNOs和Bi2WO6的紫外~可见漫反射光谱图;
图5为实施例1中RhB溶液不同降解时间的UV~vis扫描图;
图6为不同MCNOs添加量的磁性光催化剂对10mg/L RhB的降解效果图。
具体实施方式
下面通过实施例来进一步说明本发明,但不局限于以下实施例。
实施例1:
一种磁性纳米洋葱碳掺杂钨酸铋(Bi2WO6/MCNOs)催化剂的制备方法,具体步骤如下:
首先称取1.455g硝酸铋溶于6mL 2mol/L的HNO3中形成透明溶液A,取0.495g 钨酸钠溶于6mL去离子水中形成透明溶液B;将溶液B逐滴加入溶液A中形成白色悬浊液,用NaOH调节pH至3,磁性搅拌30min;再称取0.19g MCNOs加入到表面活性剂乙二醇中,超声分散30min,形成MCNOs分散液;将分散好的MCNOs分散液加入上述调好pH的悬浊液中,磁性搅拌30min形成前驱体;接着将前驱体转入带有聚四氟乙烯内衬的高温高压反应釜中,150 ºC下水热反应2h;待反应釜冷却到室温后,取反应釜中的产物,用去离子水和无水乙醇各清洗3次,然后在80 ºC下干燥8h后即可得到磁性Bi2WO6/MCNOs光催化剂。
配制10mg/L的罗丹明B 200mL,然后加入0.2g Bi2WO6/MCNOs磁性光催化剂,避光条件下超声分散10min后磁力搅拌20min达到吸附平衡;之后采用300W氙灯并加420 nm滤光片作为可见光源,反应时间为120min,每隔20min取一个样,离心后测其吸光度。然后以时间(t)为横坐标,去除率为纵坐标绘制曲线,反应该磁性光催化剂的降解性能(见图6),通过这种方法制备的催化剂在2h内对罗丹明B的降解率可达91.1%。
图1所示为Bi2WO6/MCNOs、MCNOs和Bi2WO6的XRD图谱,通过与标准卡片(PDF No. 73~1126)对比可知,Bi2WO6/MCNOs和Bi2WO6显示了一致的晶体结构和结晶度,此外,在Bi2WO6/MCNOs的XRD图谱中发现了MCNOs的特征峰,说明MCNOs已经成功复合到Bi2WO6中。
图2为Bi2WO6/MCNOs复合物的SEM图,可以看出Bi2WO6呈现片状并有较好的分散性能。
图3为Bi2WO6/MCNOs、MCNOs的磁滞回线,从图中可以看出两种样品都具有良好的超顺磁性,说明外加磁铁就可以达到磁性分离复合物的目的。
图4为Bi2WO6/MCNOs、MCNOs和Bi2WO6的紫外-可见漫反射光谱图,Bi2WO6光吸收边约为445nm,可知Bi2WO6的禁带宽度为2.75eV。此外,Bi2WO6/MCNOs复合物在可见光区域对光有更大的吸收,可以加快光生电子-空穴的产生。
图5是RhB溶液不同降解时间的UV~vis扫描图,随着反应的进行,554nm处的峰强度逐渐减弱,并发生蓝移,溶液的颜色也由玫瑰红逐渐变至无色,说明RhB被降解完成。
图6为不同MCNOs添加量的磁性光催化剂对10mg/L RhB的降解效果图,表明,当MCNOs添加量为18wt%时,催化剂对RhB的降解效果达到最大,具体含义在以下实施例中均有说明。
实施例2:
首先称取1.455g硝酸铋溶于6mL 2mol/L的HNO3中形成透明溶液A,取0.495g 钨酸钠溶于6mL去离子水中形成透明溶液B;将溶液B逐滴加入溶液A中形成白色悬浊液,用NaOH调节pH至3,磁性搅拌30min;再称取0.17g MCNOs加入到表面活性剂乙二醇中,超声分散30min,形成MCNOs分散液;将分散好的MCNOs分散液加入上述调好pH的悬浊液中,磁性搅拌30min形成前驱体;接着将前驱体转入带有聚四氟乙烯内衬的高温高压反应釜中,150 ºC下水热反应2h;待反应釜冷却到室温后,取反应釜中的产物,用去离子水和无水乙醇各清洗3次,然后在80 ºC下干燥8h后即可得到Bi2WO6/MCNOs磁性光催化剂。
配制10mg/L的罗丹明B 200mL,然后加入0.2g Bi2WO6/MCNOs磁性光催化剂,避光条件下超声分散10min后磁力搅拌20min达到吸附平衡;之后采用300W氙灯并加420 nm滤光片作为可见光源,反应时间为120min,每隔20min取一个样,离心后测其吸光度。然后以时间(t)为横坐标,去除率为纵坐标绘制曲线,反应该磁性光催化剂的降解性能(见图6),通过这种方法制备的催化剂在2h内对罗丹明B的降解率可达88.6%。
实施例3:
首先称取1.455g硝酸铋溶于6mL 2mol/L的HNO3中形成透明溶液A,取0.495g 钨酸钠溶于6mL去离子水中形成透明溶液B;将溶液B逐滴加入溶液A中形成白色悬浊液,用NaOH调节pH至3,磁性搅拌30min;再称取0.15g MCNOs加入到表面活性剂乙二醇中,超声分散30min,形成MCNOs分散液;将分散好的MCNOs分散液加入上述调好pH的悬浊液中,磁性搅拌30min形成前驱体;接着将前驱体转入带有聚四氟乙烯内衬的高温高压反应釜中,150 ºC下水热反应2h;待反应釜冷却到室温后,取反应釜中的产物,用去离子水和无水乙醇各清洗3次,然后在80 ºC下干燥8h后即可得到Bi2WO6/MCNOs磁性光催化剂。
配制10mg/L的罗丹明B 200mL,然后加入0.2g Bi2WO6/MCNOs磁性光催化剂,避光条件下超声分散10min后磁力搅拌20min达到吸附平衡;之后采用300W氙灯并加420 nm滤光片作为可见光源,反应时间为120min,每隔20min取一个样,离心后测其吸光度。然后以时间(t)为横坐标,去除率为纵坐标绘制曲线,反应该磁性光催化剂的降解性能(见图6),通过这种方法制备的催化剂在2h内对罗丹明B的降解率可达89.4%。
实施例4:
首先称取1.455g硝酸铋溶于6mL 2mol/L的HNO3中形成透明溶液A,取0.495g 钨酸钠溶于6mL去离子水中形成透明溶液B;将溶液B逐滴加入溶液A中形成白色悬浊液,用NaOH调节pH至3,磁性搅拌30min;再称取0.13g MCNOs加入到表面活性剂乙二醇中,超声分散30min,形成MCNOs分散液;将分散好的MCNOs分散液加入上述调好pH的悬浊液中,磁性搅拌30min形成前驱体;接着将前驱体转入带有聚四氟乙烯内衬的高温高压反应釜中,150 ºC下水热反应2h;待反应釜冷却到室温后,取反应釜中的产物,用去离子水和无水乙醇各清洗3次,然后在80 ºC下干燥8h后即可得到Bi2WO6/MCNOs磁性光催化剂。
配制10mg/L的罗丹明B 200mL,然后加入0.2g Bi2WO6/MCNOs磁性光催化剂,避光条件下超声分散10min后磁力搅拌20min达到吸附平衡;之后采用300W氙灯并加420 nm滤光片作为可见光源,反应时间为120min,每隔20min取一个样,离心后测其吸光度。然后以时间(t)为横坐标,去除率为纵坐标绘制曲线,反应该磁性光催化剂的降解性能(见图6),通过这种方法制备的催化剂在2h内对罗丹明B的降解率可达83.5%。
实施例5:
首先称取1.455g硝酸铋溶于6mL 2mol/L的HNO3中形成透明溶液A,取0.495g 钨酸钠溶于6mL去离子水中形成透明溶液B;将溶液B逐滴加入溶液A中形成白色悬浊液,用NaOH调节pH至3,磁性搅拌30min;再称取0.11g MCNOs加入到表面活性剂乙二醇中,超声分散30min,形成MCNOs分散液;将分散好的MCNOs分散液加入上述调好pH的悬浊液中,磁性搅拌30min形成前驱体;接着将前驱体转入带有聚四氟乙烯内衬的高温高压反应釜中,150 ºC下水热反应2h;待反应釜冷却到室温后,取反应釜中的产物,用去离子水和无水乙醇各清洗3次,然后在80 ºC下干燥8h后即可得到Bi2WO6/MCNOs磁性光催化剂。
配制10mg/L的罗丹明B 200mL,然后加入0.2g Bi2WO6/MCNOs磁性光催化剂,避光条件下超声分散10min后磁力搅拌20min达到吸附平衡;之后采用300W氙灯并加420 nm滤光片作为可见光源,反应时间为120min,每隔20min取一个样,离心后测其吸光度。然后以时间(t)为横坐标,去除率为纵坐标绘制曲线,反应该磁性光催化剂的降解性能(见图6),通过这种方法制备的催化剂在2h内对罗丹明B的降解率可达76.8%。
Claims (9)
1.一种磁性纳米洋葱碳负载Bi2WO6的光催化剂,其特征在于:以Bi2WO6为活性组分,以磁性纳米洋葱碳为载体,将Bi2WO6活性组分负载在磁性纳米洋葱碳载体上形成;该催化剂包括以下重量百分比的组分:
磁性纳米洋葱碳MCNOs:10~20wt%,
Bi2WO6:80~90 wt%;
所述的磁性纳米洋葱碳负载Bi2WO6的光催化剂的制备方法,包括以下步骤:
(1)将Bi(NO3)3·5H2O溶于硝酸中形成透明溶液A,溶液A的浓度为2.5-3.5mmol/L,再将Na2WO4·2H2O溶于去离子水中形成透明溶液B,溶液B的浓度为1.25-1.75mmol/L,其中,将Bi(NO3)3·5H2O与Na2WO4·2H2O的摩尔比为1.5:1~2:1;
(2)将溶液B以1~2mL/min的速度逐滴加入到溶液A中,形成白色悬浊液,用NaOH调节pH,磁性搅拌25~35min;
(3)取0.11~0.21g MCNOs加入到30~50mL表面活性剂中,超声分散25~35min,形成MCNOs分散液;
(4)将分散好的MCNOs分散液加入步骤(2)所得的悬浊液中,磁性搅拌25~35min;
(5)将上述溶液转入有聚四氟乙烯内衬的高温高压反应釜中,在烘箱中进行水热反应;
(6)待反应釜冷却到室温后,取反应釜中的产物,用水和无水乙醇交替清洗、离心、干燥后,即得到磁性Bi2WO6/MCNOs催化剂。
2.根据权利要求1所述的磁性纳米洋葱碳负载Bi2WO6的光催化剂,其特征在于:步骤(2)中的pH应调节至1~3。
3.根据权利要求1所述的磁性纳米洋葱碳负载Bi2WO6的光催化剂,其特征在于:步骤(3)中所述MCNOs的量应为理论Bi2WO6质量的10~20%。
4.根据权利要求1所述的磁性纳米洋葱碳负载Bi2WO6的光催化剂,其特征在于:所述表面活性剂为乙二醇。
5.根据权利要求1所述的磁性纳米洋葱碳负载Bi2WO6的光催化剂,其特征在于:步骤(5)中所述的水热反应温度即烘箱温度设置为140~180°C,反应时间为1~6h。
6.根据权利要求1所述的磁性纳米洋葱碳负载Bi2WO6的光催化剂,其特征在于:步骤(6)中所述的清洗即为用去离子水和无水乙醇交替清洗3~5次;离心转速为6000~8000r/min,离心时间为8~10min;干燥方式为烘箱干燥,温度设置在60~80°C,干燥时间为6~8h。
7.一种权利要求1所述的磁性纳米洋葱碳负载Bi2WO6的光催化剂在可见光条件下催化降解有机染料中的应用。
8.根据权利要求7所述的应用,其特征在于:所述有机染料为罗丹明B,降解过程中,罗丹明B的浓度为10mg/L,Bi2WO6/MCNOs催化剂的投加量为1.0~1.5g/L。
9.根据权利要求8所述的应用,其特征在于:所述的Bi2WO6/MCNOs催化剂对有机染料罗丹明B的去除率在2h内达80%以上。
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